HRID58171
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of [2-(3-fluoro-4-nitro-phenyl)-vinyl]-dimethyl-amine (1.7 g, 8 mmol) in MeOH, was added NaBH3CN (770 g, 12 mmol) and one drop of AcOH. The reaction mixture was stirred at room temperature for 2 hours and quenched with water. After removal of all volatiles in vacuo, the residue was extracted with 10% methanol in DCM twice. The combined extracts were washed with brine, dried over anhydrous sodium sulfate. Concentration under vacuum gave a crude product, which was purified by reverse phase column to afford the title compound (1.08 g, yield: 63%). MS (ESI): 213 [M+H]+
WORKUP
后处理
- customquenched with water
- customAfter removal of all volatiles in vacuo
- extractionthe residue was extracted with 10% methanol in DCM twice
- washThe combined extracts were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationConcentration under vacuum
- customgave a crude product, which
- customwas purified by reverse phase column